Process for the production of light voluminous oxids specially suitable for catalytic reactions.



UNITED STATES PATENT OFFICE.

FRED BEDFORD, OF SLEAFORD, ENGLAND, AN'D ERNST ERDMA NN, OF HALLE-ON-THE- SAALE, GERMANY, ASSIGNORS, BY MESNE ASSIGNMENTS, TO THE HYDROGENATION COMPANY, OF CINCINNATI, OHIO, A CORPORATION OF OHIO.

PROCESS FOR THE PRODUCTION OF LIGHT VOLUMINOUS OXIDS SPEGIALLE SUITABLE FOR CATALYTIC REACTIONS.

No Drawing.

To all whom it may concern:

Be it known that we, FRED BnDroRo, a subject of the King of Great Britain and Ireland, and ERNST ERDMANN, a subject of the Emperor of Germany, residing at Sleaford, in the county of Lincoln, England,

cordingto which the metallic oxid is. produced in a form in which it is found to be an extremely eflicient catalyst.

It is well known that in the case of metallic catalyzers, for example, nickel, cobalt,

, iron and copper, the state of fine division has a great influence upon the catalytic activity, and the same is also true of the oxids, the degree of catalytic activity of which depends not only upon the chemical quality of the oxid but also essentially upon its physical properties.

We have found that metallic oxids can be produced in an extremely finely divided and voluminous form by preparing a concentrated aqueous solution of a nitrate, mixing the same with an organic compound, preferably one which is soluble in Water and rich in carbon and subsequently decomposing by heat. A strong evolution of gas takes place during the combustion of the organic substance with the nitrate whereby the me-Q tallic oxid swells up to a large volume and assumes the form of a dust while the whole of the carbon present in the organic compound is removed by the combustion. -On reducing with hydrogen at a high temperature, preferably 200 to 300 degrees, the metallic oxids prepared according to our invention can be converted into the corre sponding voluminous and catalytically active metals, which are more eflicient thancatalytic metals prepared ,by known processes. I

Example: Nitric acid'of specific gravity of 1A2 is diluted with. an equal volume of Specification of Letters Patent. 7

Patented Oct. 10, 1916.

Application filed. November 12, 1912. Serial no. 730, 68.

water and to the diluted acid pure metallic nickel is added. When the resulting reaction is completed the whole is heated to boiling for about tfwo hours in the presence of an excess of nickel in order .to neutralme completely the nitric acid present and to precipitate any iron which may occur as hydrated oxid of iron. The clarified nickel nitrate solution is evaporated until its specific gravity is 1.6 and for each liter of this liquid (corresponding to 250 grams of nickel) "are stirred in 180. grams of pow 'dered cane sugar. portions into a mufile of any suitable construction heated to a dull red heat and the heating of each portion is continued until no more fumes escape. The voluminous nickel oxid thus formed is removed from This solution is run in the mufiie by means of a scraper and a 7 fresh portion of thesolution run in.

By means of the process, according to our invention, cobalt oxid, iron oxid and other oxids of the heavy metals which may be used for catalytic purposes, can duced in a light voluminous and catalytically active form and are extremely well adapted both in the form of oxid and in the form of metal for the process of adding hydrogento unsaturated organic compounds. I

We do not desire to confine our invention to any particular method of heating the metallic nitrate solution and organic compound, nor is the'invention to be limited to the exact proportions hereinbefore given by way of example nor to any particular organic compound with which the metallic nitrate solution is to be heated as we may emloy other forms of sugar or starch, dextrin, gum arabic, tartaric acid or other suitable organic substances, but preferably such as are soluble in water and rich in carbon.

. What we claim as our invention and desire to secure by Letters Patent is 1. A process of preparing finely-divided heavy metal oxids suitable for use as catalysts, which consists in mixing the nitrate of a heavy metal, in concentrated solution and without-admixture with other salts of the said metal, with an organic substance soluble in water and rich in carbon, and subsequently completely decomposing the organic substance by heat, whereby the be pro- I tinued until complete combustion has taken extreme subdivision.

heavy metal oxid is obtained in a state of 2. A process for the'preparation of very voluminous and light metallic oxids par- "ticularly suitable for catalytic reactions which consists in mixing the nitrate of the metal whose oxidis to be produced without admixture of other salts in concentrated s0- lution with an organic compound, soluble in place, whereby at the end of the process 15 there remains-only a metal oxid in an extremely fine state of division.

In testimony whereof, we afiix our signatures in presence of two witnesses.

FRED BEDFORD. ERNST ERDMANN.

J Witnesses to signature of Fred Bedford:

' P. A. OUTHWAITE, I J. PHILLIPS CRAWLEY. Witnesses to signature of Ernst Erdmann:

RUDOLPH FRioKn, Dome KRAHL. 

